Purification of fatty substances



(No Model.)

J. MASSIGNON. PURIFICATION OF FATTY SUBSTANCES.

No. 481,502. Patented Aug. 23,1892.

Ingre 72 29 7;

B a My? ,ktJ yd! NITED STATES PATE T FFICE.

JULES MASS'IGNON, F PARIS, FRANCE, ASSIGNOR ro THE sooIE'rE ANONYME DES PARFUMS NATURELS DE CANNES, OF SAME PLACE.

- PURlFlCATlON OF FATTY SUBSTANCES.

SPECIFICATION forming part of Letters Patent No. 481,502, dated August 2 3, 1892. Application filed June 13, 1891. Serial No. 396,1l9. (No specimens.)

To all whom it may concern.-

Be it known that -I, J ULES MASSIGNON, a citizen of the Republic of France, residing in the city of Paris, France, have inventedcertain 5 new and useful Improvements in the Purification of Fatty Substances Extracted by Volatile Solvents, of which I do hereby declare the following is a true, clear, and exact description.

o The present invention has for its object the complete separation from fatty substances of the volatile solvents that have been employed in treating the same. 1

Heretofore it has been common to drive off the solvent by evaporation, using steam-heat and reduced pressure in the evaporating-ves sel, and while these methods result in the removal of the great bulk of the solvent the last traces thereof (whose presence renders the p fatty substance of little or no value) are very difficult to remove. Moreover, in treating the fatty substance with jets of steam in the usual way there is more or less condensation, necessitating another operation to remove the water. According to the present invention, the

elimination of the solvent and water is accomplished by evaporation in vacuo until ebullition ceases, then injecting dry steam in fine jets, maintaining the temperature of the fatty 3o substance above the boiling-point of water.

In order that. the invention may be more fully understood, I will describe the operation in detail, reference being had to the accompanying drawing, which illustrates in longi- 3 5 tudinal sectional elevatio'n apparatus suitable for use in practicing the processs.

The said apparatus composed of a cylindrical boiler C contains a steam coil-pipe S to heat the interior thereof, and at its side said 40 boiler is provided with vapor-injectors I for the purpose of introducing jets of steam. At one end the boiler is provided with a series of valves A, enabling the material under treatment to be sampled from time to time. Glass 5 covered inspection-openings G G permit the condition of the material to be observed from the outside. A- dome V, mounted upon the body of the boiler, forms asafety vessel and shows any priming which might be caused in case. of the emulsion of the material. A pipe leadsfrom the dome to the coil contained in the refrigerator R, the other end of said coil discharging into a receptacle Q, with which a vacuum-pump P communicates The fatty mass containing the water and solvent is i-ntroduced into the boiler through the'mauhole G beneath the opening G, and the heat exerted by the coil S will vaporize the solvent and water and drive olf the same to the dome and condenserforseparation. 'lhevaporadmitted 6c through the injectors I effects the evaporation" of a largeportion of the solvent and its separation from the fatty body. The condenser R concentrates the solvent, after which it is passed into the receptacle Q for further treat- 6 ment. Samples are taken from time to time by means of the valves A,and vhen it is seen that the solvent has been completely eliminated the ope'i'ation is at an end. The vacuumpumpP and the injectors I maintain the nec- 7o essary relative temperature throughout the operation. Evaporation of the solution being completed in the vacuum there is at a given moment no more ebullition of the solvent, although the matter still contains an appreciable quantity. This period is readily determined, first, by the appearance of the material as seen through the inspection-openings and also because as the heating continues the temperature rises,while at the same time the degree of pressure diminishes. It is at this time that I apply my method of purificationto completely eliminate all traces of the solvent without introducing water into the fatty substances, and it is for this purpose that the 4 possible is introduced into the mass by one or several streams, this steam being under a high pressures (Thus steam escaping from the steam-motor can easily-be utilized for this purpose.) It is useful, however, that the steam jet or jets be applied in a manner to produce energetic stirring in the fatty mass, so as to 5 bring all particles of the mass into contactwith the steam. This result can be easilyobtained by the use of injectors. The steam thus injected into the apparatus not only does not condense, but the particles of water which we the boiling-point of water in the vacuum, as

already explained. This condition is essential, because without it the mass would cbol ofi'first, by the volatilization of the solvent;

second, by the evaporation of the drops of water always borne by the steam whatever care be taken to free it before its entry into the apparatus and which results, also, from the relaxation of pressure of the steam at the moment of introduction into the vessel 0.

The operation is governed by the following considerations: First, the temperature of the fatty mass in the interior of the apparatus is' in nocase to be higher than the point at which the fatty body is susceptible to-change; second, this temperature being determined regulates, also, that of the steam, which must be some degrees lower than thatiof the' fatty mass; third, the temperature of the steam-flxesthe degree of the vacuum at which the operation is to be conducted by virtue of the law of vari-.

ation of the boiling-point of any liquid with body and the steam intheinterior of the apparatus must be so much larger and the vacuum so much the greater as the boiling-point of the solvent is raised. This diflference must also be increased in inverse proportion .to the densation of this latter;

than 100 centigrade, to expand the steam eutering into the double bottom by making therein a vacuum suflicient to insure that in 40 no case will the temperature of the side heated by this double attain the temperature at which that fatty body would undergo an alteration; Under these conditions the steam acts on the fatty bodyin the apparatus like a gas, but a 45 gas which condenses afterward in a condenser at the same time as the vapors of the solvent and does not binder in any manner the ,con-T I claimt r 50 p The described processot separating volatile solvents from fatty substances by evaporating the solvent in a vacuum or rarefied medium until ebullition ceases, then injectingv dry steam in jets into the body of the substance and maintaining the latter during the'operation at a temperature above the boiling-point'of water under the conditions prescut and above the temperature of the'injected steam,as setforth.

In testimony whereof I have "signed this specification in the presence of two subscribin'g' witnesses.

JULES MASSIGNON. Witnesses: I

ROBERT M. HOOPER,\ JOSEPH TOURNIER. I 

